CN1732074A - 料坯,其生产方法,和从该料坯制造的双轴拉伸容器 - Google Patents
料坯,其生产方法,和从该料坯制造的双轴拉伸容器 Download PDFInfo
- Publication number
- CN1732074A CN1732074A CNA2003801078662A CN200380107866A CN1732074A CN 1732074 A CN1732074 A CN 1732074A CN A2003801078662 A CNA2003801078662 A CN A2003801078662A CN 200380107866 A CN200380107866 A CN 200380107866A CN 1732074 A CN1732074 A CN 1732074A
- Authority
- CN
- China
- Prior art keywords
- material base
- resin
- polyester resin
- mylar
- compression molding
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 229920005989 resin Polymers 0.000 claims abstract description 62
- 239000011347 resin Substances 0.000 claims abstract description 62
- 238000000748 compression moulding Methods 0.000 claims abstract description 43
- 229920001225 polyester resin Polymers 0.000 claims abstract description 36
- 239000004645 polyester resin Substances 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims description 114
- 229920000728 polyester Polymers 0.000 claims description 36
- 229920002799 BoPET Polymers 0.000 claims description 30
- 239000005041 Mylar™ Substances 0.000 claims description 30
- 238000001125 extrusion Methods 0.000 claims description 27
- 239000013078 crystal Substances 0.000 claims description 15
- FYIBGDKNYYMMAG-UHFFFAOYSA-N ethane-1,2-diol;terephthalic acid Chemical group OCCO.OC(=O)C1=CC=C(C(O)=O)C=C1 FYIBGDKNYYMMAG-UHFFFAOYSA-N 0.000 claims description 10
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- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 abstract description 26
- 238000002425 crystallisation Methods 0.000 abstract description 13
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- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 4
- 229920002647 polyamide Polymers 0.000 description 4
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- 239000004840 adhesive resin Substances 0.000 description 3
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- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
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- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
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- 229910052760 oxygen Inorganic materials 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
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- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
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- VIAMIUDTTIDZCA-ODZAUARKSA-N (z)-but-2-enedioic acid;propane-1,2,3-triol Chemical compound OCC(O)CO.OC(=O)\C=C/C(O)=O VIAMIUDTTIDZCA-ODZAUARKSA-N 0.000 description 1
- QVLAWKAXOMEXPM-UHFFFAOYSA-N 1,1,1,2-tetrachloroethane Chemical class ClCC(Cl)(Cl)Cl QVLAWKAXOMEXPM-UHFFFAOYSA-N 0.000 description 1
- 229920001634 Copolyester Polymers 0.000 description 1
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- 206010037660 Pyrexia Diseases 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- ORLQHILJRHBSAY-UHFFFAOYSA-N [1-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1(CO)CCCCC1 ORLQHILJRHBSAY-UHFFFAOYSA-N 0.000 description 1
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- 235000011037 adipic acid Nutrition 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 125000002723 alicyclic group Chemical group 0.000 description 1
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- QYQADNCHXSEGJT-UHFFFAOYSA-N cyclohexane-1,1-dicarboxylate;hydron Chemical compound OC(=O)C1(C(O)=O)CCCCC1 QYQADNCHXSEGJT-UHFFFAOYSA-N 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
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- 238000002156 mixing Methods 0.000 description 1
- KYTZHLUVELPASH-UHFFFAOYSA-N naphthalene-1,2-dicarboxylic acid Chemical class C1=CC=CC2=C(C(O)=O)C(C(=O)O)=CC=C21 KYTZHLUVELPASH-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
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- B29C49/0685—Compression blow-moulding
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- B29B11/00—Making preforms
- B29B11/06—Making preforms by moulding the material
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- B29C43/32—Component parts, details or accessories; Auxiliary operations
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Abstract
一种料坯和从该料坯通过拉伸成形形成的容器。该料坯有至少一层包含聚酯树脂,而且是通过压塑形成的。该包含聚酯树脂的层达到210℃等温结晶热量最大值所需要的时间是300秒或更长。从而抑制了该树脂在生产该料坯的成形期间免于发生热解。从而有效地抑制该料坯免于发生比浓对数粘度降低或产生乙醛。可以提供机械强度和香味保留优异的双轴拉伸容器。
Description
技术领域
本发明涉及一种有一个聚酯层的单层或多层料坯,涉及该料坯的生产方法,和涉及通过该料坯的双轴拉伸吹胀成形得到的容器。更具体地说,本发明涉及一种抑制了聚酯树脂热分解和大幅减少了残留乙醛的料坯,和涉及通过该料坯双轴拉伸吹胀成形得到的、有优异机械强度和香味保留性能的双轴拉伸容器。
背景技术
拉伸吹胀成形塑料容器、尤其双轴拉伸聚酯容器,由于其优异的透明度和适度的气体阻透性能,现已普遍用于这样的用途例如盛放液体例如液体洗涤剂、香波、化妆品、酱油、调料等,以及盛放碳酸饮料例如啤酒、coke(焦炭)、苹果汁、果汁、矿泉水等。
双轴拉伸聚酯容器是用如下方法成形的:通过聚酯树脂的注塑成形,事先形成一种无定形聚酯的料坯,使其底部尺寸大大小于最终得到容器的尺寸;使该料坯在拉伸温度预热;在吹胀金属模型的轴向上使该料坯张力拉伸;和在圆周方向上使该料坯吹胀拉伸(见例如JP-A-4-154535)。
有该底部的料坯的形状包括:对应于该容器的嘴和颈部分的嘴和颈部分,和要拉伸吹胀成形的、有一个底部的圆筒部分,该形状通常整体上像一支试管的形状。该嘴和颈部分形成啮合手段,以便与密封用开放端或与盖啮合。从注塑成形的必要性来看,还一定要形成一个浇口部分,以便从底部的中心朝外露出。通过树脂的压塑成形生产有底部的料坯是已经知道的。即,已经有人提出了一种料坯生产方法:切割和固定从挤塑机挤出的熔融树脂料,将其进料到一个阴模中,通过将一个阳模压嵌到该阴模中而使该料坯在该阴模中压塑成形(JP-A-2000-280248)。
然而,在通过注塑成形生产该料坯时,该熔融塑化树脂是通过喷嘴、注道、流道和浇口注入一个腔体中的。即,该树脂在该注塑成形机中长时间滞留会成为该树脂恶化的原因。具体地说,该聚酯树脂的比浓对数粘度和分子量由于热分解而降低,使得难以得到令人满意的机械强度。
进而,该聚酯树脂热分解期间产生乙醛。留在该聚酯中的乙醛变成该瓶香味保持性能恶化的原因。
发明内容
因此,本发明的一个目的是提供一种料坯,该料坯能抑制该料坯成形时该树脂的热分解并能有效地抑制比浓对数粘度的降低和乙醛的生成。
本发明的另一个目的是通过该料坯的双轴拉伸吹胀成形提供一种有优异机械强度和香味保持性能的双轴拉伸容器。
按照本发明,提供的是一种有至少一层聚酯树脂而且是通过压塑成形形成的料坯,其中,在该聚酯树脂层在210℃的等温结晶的热值达到最大值之前时间不短于300秒。
在本发明的料坯中,希望的是:
1.该聚酯树脂是以不低于95mol%的比例含有对苯二甲酸乙二醇酯的聚酯树脂;
2.该聚酯树脂含有再循环聚酯树脂;和
3.该料坯有一个除聚酯树脂层外的热塑性树脂层,具体地说,至少一个气体阻透树脂或再循环聚酯树脂的中间层以及作为内衬层和外层的聚酯树脂层。
按照本发明,进一步提供的是通过压塑成形生产一种有至少一层聚酯的料坯的方法,其中,将熔融挤塑时比浓对数粘度不小于0.72dL/g的熔融聚酯树脂进料到一台压塑成形机中压塑成形。
熔融挤塑时的比浓对数粘度即使在用压塑成形得到的料坯中或在稍后要描述的双轴拉伸容器中也没有实质性变化。
在本发明料坯的生产方法中,希望的是:
4.该熔融聚酯树脂的熔融挤塑温度在Tm+5℃~Tm+40℃范围内,并以该聚酯树脂的熔点(Tm)作为参照;和
5.熔融挤塑时的比浓对数粘度与该聚酯树脂投入该挤塑机中时的比浓对数粘度相比的降低不大于10%。
按照本发明,进一步提供一种通过该料坯的双轴拉伸吹胀成形得到的双轴拉伸容器,其中,在该聚酯层在210℃的等温结晶的热值达到最大值之前时间不短于300秒。
本发明的料坯是一种有至少一个聚酯层者而且是通过压塑成形形成的,其中,一个重要特色在于该聚酯层在210℃的等温结晶的热值达到最大值之前时间不短于300秒。如上所述,该拉伸-吹胀成形的容器的机械强度因该料坯成形时聚酯树脂热分解引起的比浓对数粘度下降而降低。
即,本发明是以如下发现为基础的:有有利结晶时间的料坯有效地抑制了该树脂的热恶化。
进而,生产了能抑制热分解的本发明料坯,从而使该料坯中剩余的乙醛数量非常少。因此,通过该料坯双轴拉伸-吹胀成形得到的拉伸-吹胀成形容器是以优异的可拉伸-吹胀成形性和香味保留性能为特色的。
在有上述结晶时间的料坯双轴拉伸-吹胀成形而得到的拉伸-吹胀成形容器中,同该料坯一样,在该聚酯层在210℃的等温结晶的热值达到最大值之前时间也不短于300秒,从而显示出优异的机械强度和香味保留性能。
图1说明当使用本发明料坯和以注塑成形法得到的惯常料坯时,从该容器体切出的样品使用差示扫描量热仪(DSC)在290℃加热熔融3分钟并保持在210℃时,在伴随结晶而出现发热峰之前的时间测定。
本发明的料坯显示出其结晶引起的发热峰宽于注塑成形法得到的料坯的结晶所引起的发热峰。进而,本发明料坯的热值达到最大值之前的时间T1可观地长于注塑成形得到的料坯的热值达到最大值之前的时间T2,由此可以理解其结晶时间可观地长于注塑成形得到的料坯的结晶时间。
即,在本发明中,重要的是,在该瓶体表面在210℃的等温结晶的热值达到最大值之前时间不短于300秒、尤其在400~700秒范围内。这一点从稍后出现的实施例的结果将变得显而易见。
例如,在有如比较例1中所证实的在该聚酯层210℃等温结晶热值达到最大值之前不长于300秒的时间的料坯中,乙醛数量是2.9μg/L。当这种料坯双轴拉伸-吹胀成形为一种瓶时,该聚酯层210℃等温结晶热值达到最大值之前的时间是250秒,且该容器体显示出低轴向弯曲强度、不良机械强度和较差香味保留性能。
另一方面,如实施例1中所证实的,在有该聚酯层210℃等温结晶热值达到最大值之前不短于300秒的时间的料坯中,乙醛量是1.9μg/g,当与比较例1的比较时,乙醛量是显著减少的。此外,当这种料坯双轴拉伸-吹胀成形为一种瓶时,该聚酯层210℃等温结晶热值达到最大值之前的时间是600秒,且该容器体显示出高轴向弯曲强度和优异香味保留性能。
如上所述,希望的是,本发明的料坯是通过将一种比浓对数粘度不小于0.72dL/g的熔融聚酯树脂进料到压塑成形机中压塑成形的。
在该料坯压塑成形时,该熔融树脂料(滴)必须输送到压塑成形位置。然而,可以拉伸和取向的结晶树脂例如聚酯树脂通常有大的垂伸趋势。因此,当增塑时,即当熔融捏合期间比浓对数粘度(IV)大大降低时,该树脂显示出由于热恶化而降低机械强度和降低香味保留性,此外,当料滴形成时发生垂伸,引起通过切割熔融树脂来获得熔融树脂料(滴)时抽丝、向压塑成形步骤输送的稳定性降低和压塑金属模型中垂直态势减少等问题。本发明抑制了树脂增塑时其热分解引起的比浓对数粘度(IV)降低并保持该树脂熔融挤塑时比浓对数粘度不低于0.72dL/g,使得有可能改进获得料滴时抽丝、向压塑成形步骤输送的稳定性和压塑金属模型中垂直态势的稳定性等问题。
附图简要说明
图1是一幅说明图,显示当使用本发明的料坯和通过注塑成形得到的惯常料坯时,且当使用差示扫描量热仪(DSC)使从容器体上切割下来的样品在290℃加热熔融3分钟并保持在210℃时,在出现伴随结晶的发热峰之前的时间测定结果;
图2是一幅视图,说明用于形成本发明料坯的压塑成形装置;
图3是一幅剖视图,说明一种按照本发明的料坯;和
图4是一幅视图,说明本发明的双轴拉伸聚酯容器。
具体实施方式
聚酯树脂
作为可以用于本发明的聚酯树脂,可以使用此前用于包装容器例如吹胀成形容器的一般热塑性聚酯树脂。具体地说,可以有利地使用对苯二甲酸乙二醇酯型热塑性聚酯。然而,也允许使用任何其它聚酯,例如聚对苯二甲酸丁二醇酯和聚萘二甲酸乙二醇酯,以及其与聚碳酸酯或聚丙烯酸酯的共混物,这是理所当然的。
在属于可以有利地用于本发明的聚酯树脂的对苯二甲酸乙二醇酯型热塑性聚酯中,大多数、尤其不少于95mol%酯重复单元是由对苯二甲酸乙二醇酯单元占据的。因此,希望的是使用玻璃化温度(Tg)为50~90℃、尤其55~80℃且熔点(Tm)为200~275℃、尤其220~270℃的热塑性聚酯。
尽管从耐热性和耐压性的观点来看均聚对苯二甲酸乙二醇酯是较好的,也允许使用含有少量除对苯二甲酸乙二醇酯单元外的酯单元的共聚酯。
作为除对苯二甲酸外的二元酸,可以使用芳香族二羧酸例如间苯二甲酸、邻苯二甲酸和萘二羧酸;脂环族二羧酸例如环己烷二羧酸;和脂肪族二羧酸例如琥珀酸、己二酸、癸二酸和十二双酸,一类单独使用或者2类或更多类组合使用。具体地说,从改善耐热性的观点来看,希望组合使用间苯二甲酸。
作为除乙二醇外的二醇成分,可以列举丙二醇、1,4-丁二醇、二甘醇、1,6-己二醇、环己烷二甲醇、和双酚A的环氧乙烷加合物,这些可以一种单独使用,也可以2种或多种组合使用。
进而,对苯二甲酸乙二醇酯热塑性聚酯可以与数量约5~约25%的、有相对高玻璃化温度的聚萘二甲酸乙二醇酯、聚碳酸酯或聚丙烯酸酯等共混使用。进而,还可以形成聚对苯二甲酸乙二醇酯和有相对高玻璃化温度的上述材料的双层。
所使用的聚酯树脂起码应当具有大到足以形成薄膜的分子量,而且因用途而异,具有注塑级或挤塑级。其比浓对数粘度(IV)通常希望当在重量比为60∶40的苯酚与四氯乙烷混合溶剂中于30℃的温度测定时在0.72~0.90dL/g、尤其0.73~0.88dL/g范围内。
其它树脂
本发明的料坯可以是仅聚酯树脂的单层料坯,也可以是有若干层除上述聚酯树脂外的热塑性树脂的多层料坯。
作为除聚酯树脂外的热塑性树脂,可以使用任何一种树脂,只要它能拉伸-吹胀成形和热结晶即可。尽管不一定仅限定于此,但其实例可以包括烯烃型树脂例如聚乙烯、聚丙烯、乙烯/丙烯共聚物、乙烯/乙烯醇共聚物和环状烯烃聚合物,和聚酰胺树脂例如含二甲苯基的聚酰胺。还可以使用通过使含二甲苯基的聚酰胺与一种双烯化合物和一种过渡金属催化剂或一种再循环聚酯(PCR(从废瓶再生的树脂)、SCR(生产装置中副产的树脂)或其混合物)共混得到的、能吸收氧的气体阻透性树脂组合物。希望的是,该再循环聚酯树脂的特性粘度(IV)当用上述测定时在0.65~0.75dL/g范围内。
再循环聚酯可以单独使用,也可以作为与新鲜聚酯的共混物使用。当再循环聚酯有降低的比浓对数粘度时,希望作为与新鲜聚酯的共混物使用它。在这种情况下,再循环聚酯与新鲜聚酯的共混比理想地是1∶5~5∶1(重量)。
进而,也可以将内层或外层经由粘合剂树脂粘附到中间层上。作为粘合剂树脂,可以使用一种用马来酸接枝聚合的酸改性烯烃树脂、一种无定形聚酯树脂、或一种聚酰胺树脂。
进而,上述聚酯树脂或除上述聚酯外的热塑性树脂还可以与各种树脂用添加剂例如着色剂、紫外线吸收剂、脱模剂、润滑剂和核化剂在它们不损害该双轴拉伸容器即最终形成的物品的品质的范围内共混。
层构造
尽管不仅限定于此,但本发明的多层料坯的层构造如以下所述。以下多层结构中的缩略语是PET:新鲜聚酯树脂;GBR:气体阻透性树脂;PCR:再循环聚酯树脂;ADR:粘合剂树脂;OAR:吸氧树脂组合物;和COC:环状烯烃共聚物。
三层结构:PET/GBR/PET,PET/PCR/PET
PET/(PET+PCR)/PET
四层结构:PET/GBR/PCR/PET
PET/GBR/OAR/PET
PET/GBR/COC/PET
五层结构:PET/ADR/GBR/ADR/PET
PET/ADR/OAR/ADR/PET
PET/GBR/PCR/GBR/PET
PET/ADR/(GBR+OAR)/ADR/PET
六层结构:PET/ADR/GBR/ADR/PCR/PET
PET/ADR/OAR/ADR/PCR/PET
七层结构:PET/PCR/ADR/GBR/ADR/PCR/PET
PET/ADR/GBR/ADR/OAR/ADR/PET
料坯成形
按照本发明,如以上所述,该料坯有一层聚酯树脂而且是用压塑成形法形成的,其中,在该聚酯树脂层210℃等温结晶热值达到最大值之前的时间不短于300秒。
在一台普通注塑成形机中,腔体是用流经热流道和浇口的树脂填充的。然而,当注塑成形机有热流道时,熔融树脂的滞留时间增加,该树脂倾向于热分解,使得难以形成有聚酯树脂层的料坯,其中该聚酯树脂层210℃等温结晶的热值达到最大值之前的时间不短于300秒。
另一方面,在压塑成形中,树脂的滞留时间短,且树脂不像注塑成形的情况下那样热劣化,这使得有可能使用通用树脂。此外,得到了这样一些优点:不形成在注塑成形中发生的会引起底部白化的浇口部分,该树脂的流动未在料坯底部取向,而且不会由于流动取向而在底部发生残留形变,从而对所形成的物品的性能影响很小。
因此,按照本发明,重要的是,该料坯是压塑成形的,具体地说,将比浓对数粘度不小于0.72dL/g的熔融聚酯树脂在熔融挤塑时进料到压塑成形机中,从而防止了该树脂的热劣化,改善了通过切割熔融聚酯树脂得到料滴时的抽丝,改善了向压塑成形步骤输送的稳定性和在压塑金属模型中垂直态势的稳定性。
在本发明料坯的生产中,希望的是,该熔融聚酯树脂的熔融挤塑温度在Tm+5℃~Tm+40℃的范围内,尤其在Tm+10℃~Tm+30℃的范围内,以该聚酯树脂的熔点(Tm)作为参照。当该温度低于上述温度范围时,剪切速度变得如此之大,以致往往变得难以形成一种均匀熔体挤塑物品。另一方面,当温度超过上述范围时,该树脂就热劣化到很大程度或发生很大程度上的垂伸,使得难以形成有以上提到的性能的料坯。
进一步希望的是,熔融挤塑时比浓对数粘度的降低,以该聚酯树脂投入该挤塑机中时的比浓对数粘度为基准,不大于10%。
图2是一幅说明用于形成本发明多层料坯的压塑成形装置的视图。在这个整体指定为1的压塑成形装置中,用于形成内层和外层的树脂A是从主挤塑机2连续进料的,而用于形成中间层的树脂B是间歇地从辅挤塑机3进料的。这两种树脂在多层模头4相遇,并从该多层模头4下面提供的喷嘴5以这样一种方式熔融挤出,使得树脂B能密封在树脂A中。挤出的所得到复合熔融树脂7由在水平方向上移动的切割手段6在没有中间层的部分切割成预定尺寸。切割后,立即用夹具将切出的复合熔融树脂的料8,并输送到由阴模9和阳模10构成的压塑成形装置的阴模9中。阴模9中复合熔融树脂的料8用阳模10压塑成形,形成一种有被内层和外层密封的中间层的多层料坯。
希望的是,本发明的料坯是使用一台能在进行压塑成形时挤塑该熔融树脂的多螺杆挤塑机形成的。这使得有可能以比使用单螺杆挤塑机时更低的温度、更低的压力和更低的速率使该树脂增塑,也有可能使该挤塑机中滞留时间的分布相对变窄,从而可以抑制增塑时该树脂的热降解,和抑制比浓对数粘度的降低以及水解引起的乙醛生成。进一步希望的是,该挤塑机配备一个通风口以使该熔融树脂中所含的水和热分解所生成的醛经由挤塑机上的通风孔强制排出,使得有可能抑制水引起的聚酯的水解,和改善该瓶的香味保留性能。
图3是一幅说明本发明的料坯当中的多层料坯的剖视图。总体上指定为20的多层料坯包括嘴和颈部分21,容器体22,和底部23。该图具体地说明通过压塑成形得到的、底部无浇口的料坯。此外,嘴和颈部分21除端部21a外有相同的三层结构,包括内层24、中间层25和外层26。
双轴拉伸容器
本发明的双轴拉伸容器是这样的:该聚酯树脂层210℃等温结晶的热值达到最大值之前的时间不短于300秒,而且是通过使本发明的料坯进行双轴拉伸吹胀成形而得到的。
在该双轴拉伸-吹胀成形中,使本发明的料坯在拉伸温度加热、在轴向上拉伸、在圆周方向上吹胀成形,从而产生该双轴拉伸容器。
料坯成形和拉伸-吹胀成形不仅能应用于冷型坯法,而且也能应用于无需完全冷却该料坯就能进行拉伸吹胀成形的热型坯法。在拉伸吹胀之前,该料坯当需要时用热风、红外线加热器或r-f电感加热等手段预热到适合于拉伸的温度。在聚酯的情况下,温度范围是85~120℃、尤其95~110℃。
将料坯进料到已知拉伸-吹胀成形装置中,固定于一个金属模具中,通过推一根拉伸杆而在轴向上张力拉伸,并通过吹流体而在圆周方向上拉伸成形。一般来说,希望的是,金属模具温度在室温~190℃的范围内。当要用稍后要描述的一次成形法(one-molding method)进行热固定时,希望将金属模型温度设定为120~180℃。
最终双轴拉伸容器的拉伸比,就面积比而言,理想地是1.5~25倍,具体地说,就轴向拉伸比而言是1.2~6倍、而就圆周方向拉伸比而言是1.2~4.5倍。
本发明的双轴拉伸容器可以用已知手段热固定。该热固定可以在吹胀成形金属模型中用一次成形法进行,也可以用两次成形法(twomolding method)在一个与吹胀成形金属模型分离的热固定金属模型中进行。该热固定温度适当地在120~180℃范围内。
作为另一种拉伸-吹胀成形方法,可以像授予本申请者的日本专利No.2917851中所公开的那样采用一种两步吹胀成形法,其中,使用一种初级吹胀金属模型将该料坯成形为一种尺寸大于最终成形物品的尺寸的初级吹胀成形体,使初级吹胀成形物品热收缩,再使用次级吹胀金属模型进行拉伸-吹胀成形,而得到最终成形物品。
图4说明本发明的双轴拉伸容器中的多层结构。在图4中,总体指定为40的双轴拉伸容器有瓶的形状,包括嘴部41、容器体42和底部43,容器体42和底部43是由内层44a、外层44b和密封在两者之间的中间层45形成的。嘴部41像以上提到的多层料坯那样,是仅由内层和外层形成的。
实施例
[DSC测定]
从料坯和从瓶体切出的样品(10mg)用差示扫描量热仪(DSC 7,Perkin Elmer公司制造)测定。
样品温度按以下顺序扫描:
1.以300℃/min的速度从室温升至290℃;
2.在290℃保持3分钟进行熔融;
3.以300℃/min的速度迅速冷却到210℃;和
4.保持在210℃,从而进行等温结晶;
并在以上4中测量时间,直至结晶热值达到最大值。
当要测定的样品是新鲜聚对苯二甲酸乙二醇酯和再循环的聚酯树脂的共混物或多层时,时间测量直至达到新鲜聚对苯二甲酸乙二醇酯树脂结晶的最大峰值,因为新鲜聚对苯二甲酸乙二醇酯以缓慢的速率进行结晶。
[IV(比浓对数粘度)测定]
在单层的情况下,从成形前的粒料切出的和从单层瓶体切出的小片状物用来作为样品。
在多层的情况下,从PET和PCR以成形时的层构成比例的混合物切出的和从多层瓶体切出的小片状物用来作为样品。溶剂是苯酚/四氯乙烷=5/5(wt)的混合物,比浓对数粘度是在30℃测定的。
关于IV(比浓对数粘度)的测定,熔融挤塑时的比浓对数粘度,与压塑成形得到的料坯的比浓对数粘度或与双轴拉伸容器的比浓对数粘度并无实质性差异。因此,使用从瓶体切出的小片状物作为样品。
[纵向压缩强度的测定]
当以50mm/min的速度压缩空瓶时,测定负荷传感器的最大负荷。
[乙醛量的测定]
一个瓶子用氮气吹扫、密封、在22℃保存一天,用气相色谱分析实测该瓶中乙醛的浓度。
实施例1
聚对苯二甲酸乙二醇酯树脂(5015W,Shinkogosen Co.制造,含98.0mol%对苯二甲酸乙二醇酯单元,熔点244℃,比浓对数粘度0.83)喂入一台挤塑机的料斗中,在模头部分的温度为270℃、树脂压力为70kgf/cm2、熔融挤塑时熔融聚酯树脂的比浓对数粘度为0.78dL/g的条件下挤塑,并切割成熔融树脂体。
将该熔融树脂体固定到保持在20℃的压塑金属模型中,在模型紧固压力为100kgf/cm2的条件下压塑成形,形成一种单层料坯。
所得到的料坯在110℃的拉伸温度加热,在保持在25℃的金属模型中双轴拉伸吹胀成形,得到一种重量25g、容积530ml的瓶子。
所形成的料坯进行DSC测定,并测定瓶子的DSC、压缩强度、拉伸强度和醛含量。
实施例2
按照与实施例1中相同的方式形成料坯和瓶子,但用聚对苯二甲酸乙二醇酯树脂(J125T,Mitsui kagaku Co.制造,含有100mol%对苯二甲酸乙二醇酯单元,熔点为254℃,比浓对数粘度为0.75dL/g)作为聚酯树脂,在这样的条件下挤塑:熔融挤塑时熔融聚酯树脂的比浓对数粘度是0.72dL/g,双轴拉伸吹胀成形中金属模型的温度设定为150℃,并在该金属模型中进行热固定,按照与实施例1中相同的方式评估。
实施例3
将一种聚对苯二甲酸乙二醇酯树脂(5015W,Shinkogosen Co.制造,含有98.0mol%对苯二甲酸乙二醇酯单元,熔点244℃,比浓对数粘度0.83)喂进一台挤塑机中形成内层和外层,并将一种再循环聚酯树脂(小片状,Yono PET Bottle Recycle Co.制造)喂进一台有通风孔的双螺杆挤塑机中形成一个中间层。这些树脂以如下方式共挤塑:该再循环聚酯树脂在模头温度为270℃、树脂压力为70kgf/cm2、熔融挤塑时熔融聚酯树脂的比浓对数粘度为0.74dL/g的条件下用聚对苯二甲酸乙二醇酯树脂密封,并切割成熔融树脂料。
将该熔融树脂料固定到保持在20℃的压塑金属模型中,在模型紧固压力为100kgf/cm2的条件下多层压塑成形,形成一种有再循环聚酯树脂中间层的两类三层料坯。
所得到的料坯在110℃的拉伸温度加热,在保持在25℃的金属模型中进行双轴拉伸吹胀成形,得到一种重量为25g、中间层比例为25wt%、容积为530ml的两种三层瓶。
测定所形成料坯的DSC,并测定该瓶的DSC、压缩强度、拉伸强度和醛含量。
比较例1
按照与实施例1中相同的方式形成料坯和瓶子,但使用注塑成形机在这样的条件下进行:注嘴温度是280℃,树脂压力是250kgf/cm2,熔体注入时即熔融挤塑时熔融聚酯的比浓对数粘度是0.71dL/g,并以相同方式评估。
比较例2
按照与实施例2中相同的方式形成料坯和瓶子,但使用注塑成形机在这样的条件下进行:注嘴温度是295℃,树脂压力是250kgf/cm2,熔体注入时即熔融挤塑时熔融聚酯的比浓对数粘度是0.67dL/g,并以相同的方式评估。
比较例3
按照与实施例3中相同的方式形成料坯和瓶子,但使用配备用于形成内层和外层的注料器和用于形成中间层的注料器的共注塑成形机在这样的条件下进行:注嘴温度是280℃,树脂压力是250kgf/cm2,熔体注入时即熔融挤塑时熔融聚酯的比浓对数粘度是0.68dL/g,并以相同方式评估。
比较例4
按照与实施例1中相同的方式形成料坯和瓶子,但使用一台挤塑机在这样的条件下进行:模头温度是285℃,熔融挤塑时熔融聚酯树脂的比浓对数粘度是0.71dL/g,并以相同方式评估。
比较例5
按照与实施例2中相同的方式形成料坯和瓶子,但使用一台挤塑机在这样的条件下进行:模头温度是300℃,熔融挤塑时熔融聚酯树脂的比浓对数粘度是0.67dL/g,并以相同方式评估。
比较例6
按照与实施例3中相同的方式形成料坯和瓶子,但使用一台挤塑机在这样的条件下进行:模头部温度是285℃,熔融挤塑时熔融聚酯树脂的比浓对数粘度是0.70dL/g,并以相同方式评估。
以上实施例和比较例的评估结果如表1中所示。
表1
*1)层构造 | 熔点(℃) | IV(dl/g) | 料坯成形方法 | 成形温度(℃) | 吹胀金属模型的温度(℃) | |
实施例1实施例2实施例3比较例1比较例2比较例3比较例4比较例5比较例6 | PETPETPET/PCR/PETPETPETPET/PCR/PETPETPETPET/PCR/PET | 244254244244254244244254244 | 0.830.750.80*2)0.830.750.80*2)0.830.750.80*2) | 压塑压塑共压塑注塑注塑共注塑压塑压塑共压塑 | 270270270280295280285300285 | 251502525150252515025 |
注)*1PET:新鲜聚对苯二甲酸乙二醇酯
PCR:再循环聚酯
*2PET和PCR的75∶25重量比混合物的IV。
表1(续)
实施例1实施例2实施例3比较例1比较例2比较例3比较例4比较例5比较例6 | 结晶时间(sec) | 从瓶体切出的小片状物的IV(dl/g) | 纵向压缩强度(N) | 乙醛含量(μg/l) | |
料坯 | 瓶 | ||||
580395480280275277278270277 | 600350405250172245249242246 | 0.780.720.74*2)0.710.670.68*2)0.710.670.70*2) | 275250251200175186198177195 | 1.901.981.922.902.952.932.952.982.92 |
注)*1PET:新鲜聚对苯二甲酸乙二醇酯
PCR:再循环聚酯
*2PET和PCR的75∶25重量比混合物
Claims (9)
1.有至少一层聚酯树脂而且是通过压塑成形形成的料坯,其中,所述聚酯树脂层210℃等温结晶的热值达到最大值之前的时间不短于300秒。
2.按照权利要求1的料坯,其中,所述聚酯树脂是以不少于95mol%的比例含有对苯二甲酸乙二醇酯单元的聚酯树脂。
3.按照权利要求1的料坯,其中,所述聚酯树脂含有再循环聚酯树脂。
4.按照权利要求1的料坯,其中,该料坯有一个除所述聚酯树脂层外的热塑性树脂层。
5.按照权利要求4的料坯,其中,所述热塑性树脂层是一个以所述聚酯树脂层作为内层和外层的中间层,而且是至少一个气体阻透性树脂层或再循环聚酯树脂层。
6.有至少一层聚酯树脂而且是通过压塑成形形成的料坯的生产方法,其中,将熔融挤塑时比浓对数粘度不小于0.72dL/g的熔融聚酯树脂进料到一台压塑成形机中压塑成形。
7.按照权利要求6的料坯生产方法,其中,该熔融聚酯树脂的熔融挤塑温度在Tm+5℃~Tm+40℃的范围内,以该聚酯树脂的熔点(Tm)作为参照。
8.按照权利要求6的料坯生产方法,其中,与要使用的聚酯树脂投入该挤塑机中时的比浓对数粘度相比,熔融挤塑时比浓对数粘度的降低不大于10%。
9.通过权利要求1的料坯的双轴拉伸-吹胀成形得到的双轴拉伸容器,其中,该聚酯层的210℃等温结晶的热值达到最大值之前的时间不短于300秒。
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EP1876019B1 (en) * | 2005-04-08 | 2013-01-16 | Toyobo Co., Ltd. | Heat-shrinkable polyester film and heat-shrinkable labels |
ITMO20060037A1 (it) * | 2006-02-03 | 2007-08-04 | Sacmi | Preforme per ottenere contenitori e relativo contenitore |
DE102008014215A1 (de) * | 2008-03-13 | 2009-09-17 | Krones Ag | Vorrichtung zum Erwärmen von Behältnissen |
WO2010024165A1 (ja) * | 2008-08-28 | 2010-03-04 | 東洋製罐株式会社 | プリフォームの圧縮成形金型及びプリフォーム、これを用いた飲・食料品無菌充填システム及びブロー成形容器の製造方法 |
GB2478732B (en) * | 2010-03-15 | 2014-08-20 | Kraft Foods R & D Inc | Improvements in injection moulding |
WO2013172812A1 (en) | 2012-05-14 | 2013-11-21 | Bayer Materialscience Ag | Multi-layer film with improved modulus properties |
US10286635B2 (en) * | 2012-05-14 | 2019-05-14 | Covestro Deutschland Aktiengesellschaft | Multi-layer film with improved modulus properties |
JP6605312B2 (ja) * | 2015-11-27 | 2019-11-13 | 株式会社吉野工業所 | 液体ブロー成形方法 |
CA3084693A1 (en) | 2017-05-31 | 2018-12-06 | Bay Materials, Llc | Dual shell dental appliance and material constructions |
US11999141B2 (en) | 2017-05-31 | 2024-06-04 | Bay Materials, Llc. | Dual shell dental appliance and material constructions |
US10870263B2 (en) | 2017-05-31 | 2020-12-22 | Bay Materials, Llc | Dual shell dental appliance and material constructions |
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- 2003-10-23 US US10/533,301 patent/US20060127615A1/en not_active Abandoned
- 2003-10-23 KR KR1020057007634A patent/KR20050067213A/ko not_active Application Discontinuation
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DE60326995D1 (de) | 2009-05-14 |
AU2003277521B2 (en) | 2009-01-08 |
CA2504212A1 (en) | 2004-05-13 |
US20060127615A1 (en) | 2006-06-15 |
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CN100425432C (zh) | 2008-10-15 |
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